Earth-treating process and product.



M. J. WELSH. EARTH TREATING PROCESS AND PRODUCT. APPLICATION FILED JUNE 1, 1913.

1,1 32,054, Patented Mar. 16,1915.

WITNESSES %"Mwl&e BY

ATTORNEY some of the lighter or less viscous oils."

earth is in condition for UNITED STATES PATENT OFFICE.

MICHAEL J. WELSH, OI PHILADELPHIA, PENNSYLVA NIA, ASSIGNOB TO THE ATLANTIC EFINING COMPANY, 03 PHILADELPHIA, PENNSYLVANIA, A. CORPORATION OF PENNSYLVANIA.

EARTH-TREATING PROCESS AND PRODUCT.

T all whom it may concern:

Be it known that a citizen of the United States, residing purposes.

In another of its aspects my invention resides in a restoration or reclamation of the material, such as fullers earth, after it melted wax, etc.

i y invention resides in the improved material herein described, and in the process of producing the same.

I shall take the treatment of fullers earth for illustrative purposes and as the p ferred form of my invention. Florida fullers earth, for example, as it is received in e raw or fresh state is first dried, so that be granulated and screened to a sizes, such, for example, as will pass through a 15 mesh oil the free moisture, and some of the Water of constitution of the fullers earth constituents. After this calcining treatment the its first use upon oil, particularly petroleum oil. The fullers eart so calcined, may first be Specification of Letters Patent. Application filed June 7,

this purpose, scribed granu at the bottom as gives the desired results.

vantage, be employed in th clarification t e filter laced kept the filtration cosity. Or th used on such cosity or may or liquids of any grade or viscosity.

erally sure tight so that the oil acted upon as be forced thro pressure.

Patented Mar.

1913. Serial No. 772,415.

when earths of th lation are employed, a chamof the chamber of the more viscous 0118, and if these latter are of employing the fullers in a Warm at suitably high e above ded provided referg, and with ad- 0 purification or petroleum great viscosity earth may room or be otherwise temperature to assist process by reducing the vise calcined earth oils or liquids may be first great visbe continuously used on oil well as the fluids used subsequently for cleaning the fullers ugh the calcined e i'ter the fullers earth has be A or less exhausted as acting upon OllS or or liquid is discontinued and liquid still wit it. Any oil 0 drainage may And the oil or liqu d that has been it porous struc displaced by steam steam and the Water aiding in the process.

hin the r liquid remaining be driven out by The naphth blast, the h ture.

of the exhausted earth it ordinari earth ma arth under (0 H10 more to its powers for so liquids, the influx of oil the oil or earth is drained from after this contained in a is in turn eat of the yes of condensation both combustion ceases additional heat is applied to the earth with the result that the oxygen of the air enters and consumes the carbon or carbonaceous materials deposited in the earths pores. After this second calcining the fullers earth may be again used in the treatment of oils as above described; may be again cleaned and calcined, and so on, repeatedly. But it loses some of its efficiency in operating upon the oil or liquid with each handling or calcining, so that with repeated uses with subsequent treatments in the calcining kilns it either entirely loses its valuable operative properties or loses them to so great an extent that the earth is practically exhausted. This loss of efficiency is believed to be due to two causes; first the carbonaceous material is not entirely removed or burned out in each calcinin treatment; and second, and of greater importance, even with very careful handling of the earth, incipient fusion results at the calcining temperatures attained, and with the fusion of the earth it of course loses to great extent its operative properties. By m invention however I reclaim or restore ullers earth so exhausted by repeated actions upon oil or liquid and succeeding treatments in calcining kilns, by treating it with acid of suitable strength. I may use sulfuric, hydrochloric, nitric, or other suitable acid. The efi'ect of the acid upon the spent earth is to dissolve some of its constituent parts, while other constituents are disintegrated, with the result however that the efliciency is increased by the acid treatment. But the more important action of the acid is that the constituents removed are largely the alkaline earths or alkaline earth metals and other constituents which induce, or lend themselves as fluxes in producing, fusion of the earth during the calcining treatment. In other words by the acid treatment some of those materials which cause or lend themselves to the undesirable fusion of the earth, are removed, with the result that in subsequent calcining treatments there is little or no fusion and the efiiciencv of the earth is maintained or improved. In consequence the exhausted earth so treated is restored or reclaimed; or if the earth has not been completely exhausted, such acid treatment maintains or improves its efiieiency. In either case the earth can be used far oftener or in contact with more oil or liquid than in the case of the untreated earth. By my acid treatment the temperature producing destructive or undesirable amount of fusion of the treated earth is, raised considerably with respect to the fusing temperature of the untreated earth. In some cases I have found that the acid treatment raises this incipient fusion point to a good red heat as distinguished from a dull red heat for untreated earth. Acid treatment therefore puts the earth in such condition that it materially resists fusion at the temperature of and at all temperatures lower than that reached in the calcining and necessary for the destruction of and removal of the carbonaceous matter from the pores.

The treatment of the fullers earth by acid may be during a single long period or in several successive short periods. By preference however the earth is subjected to the acid in a single long treatment. It is within my invention to so treat the earth with acid more than once, each time after one or more uses upon oil succeeded by one or more calcining treatments. But a single acid treatment suflices for numerous repeated andsubsequent uses upon oil or liquid with corresponding subsequent treatments in calcining kilns. My invention may be viewed also as a treatment of the fullers earth by acid to remove the fiuxing materials, so that the earth may withstand numerous subsequent high temperature treatments in calcining furnaces or kilns without serious reduction of porosity 01* efficiency by fusion of some of its constituents.

While I have above described my preferred process as involving the use of the fullers earth upon oil or liquid before the acid treatment, it is to be understood that the acid treatment will improve the earth and render it substantially non-fusing even before use upon oils. or fresh earth is first granulated and then calcined. Then it may be treated with acid and thereafter for the first time used upon oil or liquid.

Calcining the fresh or raw earth before acid treatment is preferable because in the treatment of the fresh or raw earth by acid, before calcining, the earth disintegrates, and becomes largely nothing but mud. The chemical composition of the-fresh or raw earth is such that its structure is largely destroyed or disintegrated when it is wetted with water or aqueous solution of acid. On the other hand if the raw earth is first calcined the heat causes changes in composition, such as driving off of water of constitution, and ,other changes, and the earth has then sufficient strength of structure to admit of treatment by acid solution without losing its desired granular formor porosity. However, I may first treat the raw or fresh fullers earth with acid, thereby reducing a large proportion of it to structureless mud, thereafter washing the mud away, thereafter calcining the residue comprising material having filtering, decolorizing or purifying properties, and using the calcined residue upon oil or my preference is to calcine the granulated raw earth, then use it one or more times upon oil or liquid, and then after subsequent calcining treat it with acid.

liquid. But as outlined above That is to say, the raw It has been my experience in the treatment pipe 7, extending down into the tank T, has of lubricating oils that fullersearth becomes a revoluble air tight connection, a suitable more or less exhausted after having been ball bearing for the pipe 7 and the parts used from twelve to fifteen times, while attached thereto being provided at 8. treated fullers earth can be used economithe lower end of the pipe 7 is attached the cally more than double this number of times. pipe 9, which may be curve as shown, in

e treated earth can be used until it is deconformity with the bottom of the tank T. stroyed by the breaking down of its porous This pipe 9 has a plurality of lateral perstructure during the handling processes orations, these perforations on one side of through which it passes; that is to say, by the pipe 7 facing in one direction, and those the mechanical destruction of its structure on the other side of pipe 7 in another direcby the wearing away of its granules. It is tion, so that when water or air under presto be understood that after the acid treatsure is delivered through pipe 7 into pipe 9, ment the acid is removed from contact the water or air escapes through these aperwith the earth and the remaining acid is tures and the reaction causes the pipe 9 so thoroughly washed out, and thereafter the with its attached pipe 7 to rotate, and durclay dried before its next contact with oil. ing rotation communication is maintained esides oils, other materials in liquid or fluid with the pipe 4 through the T 6. This rostate may be operated upon by the earth, tation of the pipe 9 agitates or mixes the maand particularly, melted paraffin or other terial within the tank T, that is, the acid wax, and melted stearic acid may be so opand fuller-s earth by carrying around water erated upon. And with respect to stearic or air to different parts of the tank T. The acid treatment, it is important th t the 6 is attached to the chain or cord 11 which earth shall have been first treated; for, with passes over the top of the derrick 12 to the untreated earth, the stearic acid attacks the Windlass 13. By this Windlass pipe or agi- 9o earth, much in the manner of the mineral a r 9 may be elevated to different posiacid h reinbef re described, and its lf be tions as occasion may require. In case air comes more or less neutralized. is to be passed through the pipes 7 and 9 In t e accompanying drawing I have the valve in pipe 14 leading to the air storillustrated apparatus suitable for the h reage tank A is opened. this tank A bein inbefore described treatment of full rconnected by pipe 15 with the air pump P. earth. Steam admitted to tank T through pipe 3 In starting a treatment of the fullers raises the temperature of the mixture prefearth, acid is pumped by acid pump P erably to the boiling point. The agitation through pipe 1 into the treating tank T. is kept up for a suitable length of time 1 he acid so pumped mav be weak acid from while the mixture is kept near or at the boilthe weak acid tank A, this weak cid being ing point. The agitation may then be dis left over from a prior treat, or strong acid continued for a suitable length of time and from the strong acid tank A in which case repeated at intervals during the treatment. t e strong acid is diluted to the proper And throughout the treatment the mixture 195 strength by mixture with weak acid or with is kept at or near the boiling point as stated. water, the water being delivered by pump When it is found that the acid ceases or 1 through pipes 2, 4, 5, 6, 7 and 9. The nearly ceases to act, the operation of washdepth of the acid solution in the tank T is ing the acid from the earth is begun. For

the washing, water 15 forced by pump P amount of fullers earth to be treated. The through pipes 2 and 4 into the tank T fullers earth, preferably previously well through pipe 9 until the latter is nearly washed and steamed, is delivered by elevator filled. The contents of the tan are now into the tank T. As it is being delivered thoroughly mixed, and the earth allowed to into the acid solution in tank T t e agitation Settle. The liquid in the tank is then drawn of the mixture is begun and continued until oil through the valves and connections situall the fullers earth of the treat has been ated above the earth line in the tank, the delivered into the acid solution, and thereliquid in this operation passing off through after as long as requisite. t e draw 0 pipe 16. Preferably this Throughout the drawing the various liquid is delivered to the weak acid tank A, valves are indicated by the reference charany surplus being discharged to the sewer acter'u. It will be understood that these through pipe 17. T e washin is then convalves maybe opened and closed at will, to tinned by filling the tank T with water,m1xcontrol delivery of the materials to the ing it well with the earth, and allowing the various parts of the apparatus at various earth to settle, drawing oil the Water into times. the sewer through pipes 16 and 17. This The agitation of the mixture above re- Washing is continued until the liquid dis ferred t is accomplished by the introduccharged from the tank T is clear and free tion of air or water through pipe 4 and from acid. When the earth has been satisflexible hose 5 to the T 6 with which the factorily washed, the mass is agitated while 139 mixed with sufficient water to cause the mixture to readily flow through the bottom cock of tank T into the lower or drying tank or chamber T The water of the mixture is now drained off through the bottom of tank T. Steam from the boiler B, super-heated in the super-heater S is delivered into the tank T, now tightly closed at its top, through pipe 19. This steam is forced through the earth from above for the purpose of removing a portion of the water remaining in the earth and for heating the earth. When the earth has been so treated by steam and thoroughly heated throughout, compressed air, from tank A heated in the super-heater S, is passed through pipe 20 into the tank T through the earth. In this connection it will be understood that the tank T is provided with a perforated false bottom 21 over which is placed a filter cloth of canvas or other suitable material, the steamer air current passing through the earth and out through the false bottom. When 30 B. acid and fifty tons of earth are used in the above mentioned treatment, I have found that it requires approximately 96 hours duration of contact between earth and acid and substantially 48 hours for the washing process before the earth is ready for the drier T The earth having been treated and dried as above described, it is removed from the tank T and further dried as in kilns or calcined and is then in condition for further treatment of oil or liquid as hereinbefore described.

Pursuant to a requirement for division, I do not herein claim the treating apparatus, the method of treating or preparing raw fullers earth or earthy material of similar characteristics, nor the product resulting from such method, nor the method of prearing fullers earth or earthy material of like characteristics for action upon organic acid, such as stearic acid, nor the method of treating stearic acid, the same being claimed in my co-pending application Serial Number 4441, filed January 26, 1915.

What I claim is:

1. The method of maintaining or improving the efficiency of fullers earth or earthy material of similar characteristics rendered more or less inefficient by percolation of liquid therethrough, which consists in treating the fullers earth or earthy material with acid which dissolves or extracts ingredients of said earth or earthy material tending to produce fusion.

2. The method of maintaining or improving the efficiency of fullers earth or earthy material of similar characteristics rendered more or less inefiicient by its action on organic liquid, which consists in treating the fullers earth or earthy materialwith acid which dissolves or extracts ingredients of said earth or earthy material tending to roduce fusion.

3. The method of maintaining or improving the efficiency of fullers earth orearthy material of similar characteristics rendered more or less inefficient by its action on oily liquid, which consists in treating the fullers earth or earthy material with acid which dissolves or extracts ingredients of said earth or earthy material tending to produce fusion.

4. The method of maintaining or improving the efficiency of fullers earth or earthy material of similar characteristics rendered more or less inefficient by its action on oily liquid, which consists in treating the fullers earth or earthy material with a solvent for material extracted thereby from oily liquid, and thereafter treating said fuller-s earth or earthy material with acid which dissolves or extracts ingredients of said earth or earthy material tending to produce fusion.

5. The method of maintaining or improv ing the efliciency of fullers earth or earthy material of similar characteristics rendere more or less inefficient by its action on oily liquid, which consists in calcining said fullers earth or earthy material, and thereafter treating the same with acid which dissolves or extracts ingredients of said earth or earthy material tending to produce fusion.

6. The method of maintaining or improv' ing the efficiency of fullers earth or earthy material of similar characteristics rendered more or less inefficient by its action on oily liquid, which consists in treating said fullers earth or earthy material with a solvent for material extracted thereby from oily liquid, calcining said fullers earth or earthy material, and thereafter treating the same with acid which dissolves or extracts ingredients of said earth or earthy material tending to produce fusion.

7 The method of maintaining or improving the efiiciency of calcined fullers earth or earthy material of similar characteristics rendered more or less inefiicient by its action on oily liquid, which consists in treating the fullers earth or earthy material with acid which dissolves or extracts ingredients of said earth or earthy material tending to roduce fusion.

8. The method of maintaining or iinproving the efficiency of calcined fullers earth or earthy material of similar characteristics rendered more or less inefficient by its action onoily liquid, which consists in treating the fullers earth or earthy material with a solvent for material extracted thereby from oily liquid, and thereafter treating said fullers earth or earthy material with acid which dissolves or extracts ingredients of said earth or earthy material tending to produce fusion.

9. The method of maintaining or improvthe efficiency of calcined fuller-s earth or earthy material of similar characteristics rendered more or less inefficient by its action on oily liquid, which consists in calcining said fullers" earth or earthy material, and thereafter treating the same with acid which dissolves or extracts ingredients of said earth or earthy material tending to produce fusion.

10. The method of maintaining or improving the efliciency of calcined fuller-s earth or earthy material of similar characteristics rendered more or lessineflicient'hy its action on oily liquid, which consists in treating said fnllers" earth or earthy material with a solvent for material extracted therebyfrom oily material, calcining said fnllers earth or earthy material, and thereafter more or les ineficienti by its action on petroleum, which in treating fullers earth or earthy material with a sol rent for material extracted thereby from petroleum, and thercsftcrtr'ecting the si me acid 'which dissolvesor extracts ingredients of said earth. or earthy material tendingto produce fusion 13. The method of maintaining or improving the efliciency; of fuller-s earth or earthy material of similar characteristics rendered more or less inefiicient by its action on petrolenm,'wh ich consists in calsaid fuller-s earth or earthy material, and thereafter treating the same with acid which dissolves or extracts ingredients of saidharth or earthy material tending to produce fusion.

ii The method of maintaining or im proving the e fliciency of fuller-s can't-h or earthy material of similar characteristics rendered more or less; ineflicient by its action on petroleum, which consists in treating said fullers or earthy material with a solvent for material extracted thereby irom petrolenm, calcining said fullcrs earth or earthy material, and thereafter treating the same with acid which dissolves or extracts ingredients of said earth or earthy materal tending to produce fusion. 15. The method ofmaintaining or improving the e fliciency of fnllers" earth rendered more or less inefficient by percolation of pet-rolemn therethrongh, which consists in treating said fullers earth with acid which dissolves or extracts ingredients of said earth tending to produce fusion.

16. The method of maintaining or improving the elliciency of fullers earth or earthy mziterial of similar characteristics rendered more or less inefficient by percolation of oily liquid therethrough, which con sists in treating the fullers earth or earthymaterial with acid which dissolves or ex tracts ingredients of said earth or earthy material tending to produce fusion, and thereafter calcining the same before further percolation of oily liquid therethrough.

17. The method of preparing: fullers earth or earthy material of similarvcharam teristics jor percolation of oily liquid therethrough, which consists in treating said fullers earth or earthy material acid which dissolves or extracts ingredients of said earth or earthy material tending to produce fusion.

18. The method of preparing fullers earth or earthy material of similar characteristics for percolation of oily liquid therethrongh which consists in treating said fullers earth or earthy material with acid which dissolves or extracts ingredients of said earth or earthy material tending to produce fusion, and thereafter calcining the same.

19. The method of preparing fnllers earth or earthy material of similar characteristics for percolation of-oily li id therethrongh, which consists in calclning said fullers earth or earthy material, and thereafter treating the same with acid which dissolves or extracts ingredients of sind earth or earthy material tending to produce in- 20. The method of treating fzillers earth or earthy material of similar characpercolation of oily liquid therethrongh, which consists in treating said fnllers earth or ear'thy material with acid'torcise its fusion point, said acid disolving or extracting ingredients of said earth or earthy material tending to produce fusion, whereby said fullers earth or earthy material after subsequent percolation of oily liquid theretlu-ough may be calcincdnt red heat;

teristics rendered more or less inellicient by 21. The method of treating fullemearth or earth of similar characteristics mndene mpreor-lesineficient by percolation of oil therethro agh, whieh cens sts in alkaline therefrom.

The of 'treating' fellas earth "ozearth of charaeteris ies rend more-orlessinefiicient'h percolatimifof thereflnfngh, whieh eansists in extracting by aeid sai abi 1issolving--01 extras(5mg ingredients of said earth orearflzy material tending teproduce extras-tidal therefrong'oi constiteents inducfusien;

resixiue 0f fuflers earth remaining afterer traction therefrom of constituents inducing fusion at, red heat 26. The method of preparing fuilers earth or earthy material of similar characteristicsfor action upon oily liquid, which consists in calcining said fullers earth or earthy materiaL treating said fullers earth or earthy material with acid which dissolves or extracts ingredients of sai earth or earthy material tending to produce fusion, and thereafter calcining the same.

In testimony whereof I have hereunto afiixed my signature in the presence of the two subscribing witnesses.

MICHAEL J. "WELSH.

Witnesses:

E. J. HE'S-RY, W. M. 111511.

It is hereby certified that in Letters Patent No. 1,132,054, granted March 16, 1915, upon the application of Michael Welsh, of Philadelphia, Pennsylvania, for

.an improvement in Earth-Treating Processes and Products," errors appear in the printed specification requiring .correction as follows: Page 5, line 124, after the comma, insert the words said acid dissolving or extracting ingredients of said earth or earthy material tending to producefus'llon; page 6, lines 912 strike out the comma and the words said acid dissolving or extracting ingredients of said earth or earthy material tending to produce fusion therefrom and insert the words constituents inducingfusion 'in calcining; and that the said Letters Patent should be read with these corrections therein that the same may conform to the record of the case in the Patent Olfice.

Signed and sealed this 3rd day of August, A. D., 1915.

[SEAL] R. F. WHITEHEAD,

Acting Commissioner of Patents. 

